CN116040626A - Method for purifying reduced pressure alkali fusion graphite - Google Patents
Method for purifying reduced pressure alkali fusion graphite Download PDFInfo
- Publication number
- CN116040626A CN116040626A CN202310060640.0A CN202310060640A CN116040626A CN 116040626 A CN116040626 A CN 116040626A CN 202310060640 A CN202310060640 A CN 202310060640A CN 116040626 A CN116040626 A CN 116040626A
- Authority
- CN
- China
- Prior art keywords
- graphite
- reduced pressure
- alkali
- acid
- melted
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 121
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 99
- 239000010439 graphite Substances 0.000 title claims abstract description 99
- 239000003513 alkali Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 29
- 230000004927 fusion Effects 0.000 title description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 90
- 239000002253 acid Substances 0.000 claims abstract description 39
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 13
- 238000002844 melting Methods 0.000 claims abstract description 12
- 230000006837 decompression Effects 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000002386 leaching Methods 0.000 claims description 40
- 238000003756 stirring Methods 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- 230000007935 neutral effect Effects 0.000 claims description 8
- 230000008018 melting Effects 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000012065 filter cake Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 238000000967 suction filtration Methods 0.000 claims description 5
- 238000000605 extraction Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 abstract description 20
- 238000000746 purification Methods 0.000 abstract description 14
- 230000000694 effects Effects 0.000 abstract description 7
- 238000009792 diffusion process Methods 0.000 abstract description 4
- 238000007499 fusion processing Methods 0.000 abstract description 3
- 238000007500 overflow downdraw method Methods 0.000 abstract description 3
- 239000012466 permeate Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 10
- 239000012295 chemical reaction liquid Substances 0.000 description 8
- 239000011229 interlayer Substances 0.000 description 5
- 238000001914 filtration Methods 0.000 description 4
- 239000007770 graphite material Substances 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- 238000009210 therapy by ultrasound Methods 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 210000003000 inclusion body Anatomy 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
- C01B32/215—Purification; Recovery or purification of graphite formed in iron making, e.g. kish graphite
Landscapes
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention provides a method for purifying reduced-pressure alkali-melting graphite, and relates to the technical field of graphite purification. The invention strengthens the ordinary alkali fusion process by using a decompression alkali fusion method, improves the permeation and diffusion of the reaction solution in the graphite layer and the micropores in the graphite, can permeate the high-concentration sodium hydroxide in the graphite, improves the impurity removal effect, solves the problems of uneven mixing of the molten alkali solution and the graphite by using the ordinary alkali acid method and insufficient reaction with impurities in the graphite, and finally ensures that the fixed carbon content of the purified graphite is more than or equal to 99.9 percent. Meanwhile, the graphite purification process disclosed by the invention is simple in steps, high in purification efficiency, low in purification cost and wide in application prospect.
Description
Technical Field
The invention relates to the technical field of graphite purification, in particular to a method for purifying reduced-pressure alkali-melting graphite.
Background
The graphite has excellent performances of conductivity, heat resistance, good toughness, corrosion resistance, strong plasticity, good lubricating performance and the like, can be widely applied to various industries such as aerospace, metallurgy, machinery, electronics, national defense and the like, and is an essential strategic mineral resource for national economy. Tiantian (Chinese character of 'Tian')The graphite ore is not high in grade and contains more impurities including SiO 2 、Al 2 O 3 MgO, feO, etc., and is required to be processed and purified before application. The graphite purity determines the service performance and the comprehensive performance of the graphite deep-processing product, and the higher the graphite purity is, the higher the application value is. The purity of graphite is required to be higher than 99% for cathode materials for lithium ion batteries, raw materials for artificial diamond, flexible graphite materials for sealing heat conduction, and special graphite materials for aerospace and nuclear industries. Therefore, the purification of graphite is the basis for preparing all graphite materials, is a common problem for the development of graphite materials, and has important research significance for promoting the utilization of graphite resources in China by developing a graphite purification process with low energy consumption, less pollution and high efficiency.
The main purification methods of graphite at present comprise a flotation method, an alkali acid method, a hydrofluoric acid method, a chloridizing roasting method and a high-temperature purification method. The alkali-acid method removes impurities through the reaction of alkali, acid and impurities, has simple process operation and lower production cost, does not generate toxic and harmful wastes, and has the advantages in the industrial application of the present stage. However, since the graphite has a layered structure, the interlayer distance of the graphite is 0.335nm, the bonding force between layers is weak, and the carbon atoms in each layer of the graphite pass through sp 2 The hybridization is formed, and the symmetrical structure ensures that the surface of the hybrid fiber is weaker in polarity and is not easy to be wetted by reaction liquid with strong polarity. In addition, the embedding relationship between graphite and gangue minerals is complex, and impurities with smaller particle sizes exist in the graphite in the form of inclusion bodies, so that the inclusion bodies are difficult to completely contact with acid and alkali reaction substances and react, and the impurities in the graphite are difficult to completely remove. Finally, a large number of micropores exist on the surface of the graphite, and the gas existing in the micropores also blocks the entry of the reaction liquid, so that the permeation of the reaction liquid and the contact and impurity removal of impurities in the graphite are affected. The above reasons lead to relatively low purification efficiency and unsatisfactory impurity removal effect of the conventional alkali acid method. Therefore, how to improve the existing technology to g-dose the above-mentioned problems is a technical problem to be solved in the art.
Disclosure of Invention
In order to solve the problems, the invention improves the traditional alkali acid method by using a decompression alkali fusion process, and a decompression impregnation treatment process is arranged before alkali fusion and in the acid leaching process, and the reaction liquid is fully infiltrated and diffused between the graphite layered structure and the internal gap by using negative pressure, so that the infiltration capacity of alkali liquor and acid liquor to graphite and the infiltration amount of the reaction liquid are improved, the purification effect of alkali fusion acid leaching is effectively improved, and the method has wide application prospect.
The method for purifying the reduced pressure alkali-melted graphite specifically comprises the following steps:
(1) Adding graphite powder into a sodium hydroxide solution, heating, and then stirring by ultrasonic to enable graphite to fully contact with sodium hydroxide to obtain a mixture I;
(2) Placing the mixture I into a high-temperature furnace for air extraction and decompression, performing reduced pressure alkaline leaching, heating and drying until the moisture is completely volatilized after alkaline leaching, continuously heating and performing reduced pressure alkaline melting roasting, and washing the graphite subjected to reduced pressure alkaline melting with deionized water to be neutral to obtain a mixture II;
(3) And mixing the mixture II with acid liquor, carrying out acid leaching under the conditions of heating and stirring, carrying out suction filtration after the acid leaching is finished, recovering the acid liquor, washing a filter cake with water to be neutral, and drying to obtain the purified graphite.
Further, the concentration of the sodium hydroxide solution in the step (1) is 5-30wt%, and the weight ratio of the graphite powder to the sodium hydroxide is 1:0.6-1:0.8.
further, in the step (1), the ultrasonic stirring temperature is 40-60 ℃, the ultrasonic stirring time is 15-90min, and the ultrasonic stirring power is 200W.
Further, in the step (2), the drying temperature is 200 ℃, the alkaline leaching pressure is 0.3-0.5 atmosphere, and the alkaline leaching time is 0.5-1.5h.
Further, in the step (2), the reduced pressure alkali fusion roasting temperature is 400-600 ℃, the reduced pressure alkali fusion roasting pressure is 0.5-0.8 atmosphere, and the reduced pressure alkali fusion roasting time is 1.5-3.0h.
Further, the acid liquor in the step (3) is one or more of hydrochloric acid, nitric acid and sulfuric acid, and the concentration of the acid liquor is 1.5mol/L.
Further, in the step (3), the solid-to-liquid ratio of graphite to acid liquor is 1g to 20mL, the acid leaching temperature is 80 ℃, and the acid leaching time is 80min.
Further, the fixed carbon content of the purified graphite in the step (5) is more than or equal to 99.9 percent.
The invention adopts a decompression alkali fusion method, and increases the adhesive force between the reaction solution and the graphite under the decompression condition, so that the adhesive force is larger than the cohesive force between sodium hydroxide molecules, thereby completely attaching and wetting the sodium hydroxide on the surface of the graphite, and solving the problem of poor compatibility of a polar sodium hydroxide solution and nonpolar graphite. Under the condition of reduced pressure, gas in the interlayer and the inner micropore of the graphite escapes, a large number of gaps and channels are provided for the entering and diffusion of sodium hydroxide, so that the sodium hydroxide is sucked into the interlayer and the micropore of the graphite, the permeation and diffusion process of the sodium hydroxide is greatly improved, and the sodium hydroxide can comprehensively enter the whole inner space of the graphite to be in direct contact reaction with impurities in the graphite. In addition, under the condition of reduced pressure, when the reaction liquid is in a complete fusion state with each interlayer of the graphite and the interface of the graphite micro holes, the adsorption effect is generated, so that the reaction liquid is not only filled in the interlayer and the micro holes of the graphite, but also is tightly combined with the surface of the graphite. And meanwhile, the alkali liquor in the graphite layers and micropores is sucked under reduced pressure, and the dried sodium hydroxide and the graphite are firmly integrated into a whole along with the temperature rise and the evaporation of water. The temperature rises to reach the melting point, sodium hydroxide completely entering the graphite is slowly melted and fully contacted with impurities, and continuously reacts with the impurities in the graphite, and meanwhile, the alkali is melted under reduced pressure, so that more molten sodium hydroxide continuously enters and reacts with the impurities in the graphite, the alkali melting process is strengthened, and the impurity removing effect is improved.
Compared with the prior art, the invention has the beneficial technical effects that:
(1) The invention strengthens the ordinary alkali fusion process by using a decompression alkali fusion method, improves the permeation and diffusion of the reaction liquid in the graphite layer and the micropores in the graphite, can permeate the high-concentration sodium hydroxide in the graphite, improves the impurity removal effect, and solves the problems of uneven mixing of the molten alkali liquid and the graphite and insufficient reaction with impurities in the graphite by using the ordinary alkali acid method;
(2) The graphite purification process has the advantages of simple steps, high purification efficiency, low purification cost and wide application prospect.
Detailed Description
The invention provides a method for purifying reduced-pressure alkali-melting graphite, which comprises the following steps:
(1) Adding graphite powder into a sodium hydroxide solution, heating, and then stirring by ultrasonic to enable graphite to fully contact with sodium hydroxide to obtain a mixture I;
(2) Placing the mixture I into a high-temperature furnace for air extraction and decompression, performing reduced pressure alkaline leaching, heating and drying until the moisture is completely volatilized after alkaline leaching, continuously heating and performing reduced pressure alkaline melting roasting, and washing the graphite subjected to reduced pressure alkaline melting with deionized water to be neutral to obtain a mixture II;
(3) And mixing the mixture II with acid liquor, carrying out acid leaching under the conditions of heating and stirring, carrying out suction filtration after the acid leaching is finished, recovering the acid liquor, washing a filter cake with water to be neutral, and drying to obtain the purified graphite.
In one embodiment, the concentration of the sodium hydroxide solution in the step (1) is 5wt% to 30wt%, and the weight ratio of the graphite powder to the sodium hydroxide is 1:0.6-1:0.8.
in one embodiment, the ultrasonic stirring temperature in the step (1) is 40-60 ℃, the ultrasonic stirring time is 15-90min, and the ultrasonic stirring power is 200W.
In one embodiment, the drying temperature in step (2) is 200 ℃, the alkaline leaching pressure is 0.3-0.5 atm, and the alkaline leaching time is 0.5-1.5h.
In one embodiment, the temperature of the reduced pressure alkali fusion roasting in the step (2) is 400-600 ℃, the pressure of the reduced pressure alkali fusion roasting is 0.5-0.8 atmosphere, and the time of the reduced pressure alkali fusion roasting is 1.5-3.0h.
In one embodiment, the acid solution in the step (3) is one or more of hydrochloric acid, nitric acid and sulfuric acid, and the concentration of the acid solution is 1.5mol/L.
In one embodiment, in the step (3), the solid-to-liquid ratio of graphite to acid solution is 1g:20mL, the acid leaching temperature is 80 ℃, and the acid leaching time is 80min.
In one embodiment, the fixed carbon content of the purified graphite in step (5) is greater than or equal to 99.9%.
The technical scheme provided by the invention is further described below by combining with the embodiment.
Example 1
2.8g of sodium hydroxide is dissolved in 10mL of deionized water according to the weight ratio of graphite to sodium hydroxide of 1: adding 4g of graphite powder with the carbon content of 91% in a proportion of 0.7, heating at 50 ℃ under 200W for ultrasonic treatment for 30min, uniformly stirring, putting the graphite-containing solution into a high-temperature furnace, pumping to a decompression state, keeping 0.4atm in the first stage, and performing alkaline leaching under the decompression state for 1.5h. Heating after alkaline leaching, keeping the temperature to 200 ℃, keeping the pressure at 0.5-0.8atm, drying until the water volatilizes completely, performing alkaline leaching roasting at 500 ℃ for 120min, cooling to 50 ℃, performing magnetic stirring water leaching for 30min, performing suction filtration, washing to neutrality, drying a filter cake, adding graphite after alkaline leaching into 80ml of 1.5mol/L nitric acid solution, performing acid leaching at 80 ℃ for 80min to remove impurities in the graphite, performing suction filtration, washing to neutrality, and drying to obtain a finished product. The fixed carbon content of the graphite finished product reaches 99.94 percent.
Comparative example 1
The difference from example 1 is that: the fixed carbon content of the obtained graphite finished product is 99.08% without adopting reduced pressure alkali fusion.
Example 2
3.2g of sodium hydroxide is dissolved in 10mL of deionized water, and the mass ratio of graphite to sodium hydroxide in the prepared alkali liquor is 1:0.8 g of graphite powder with a carbon content of 91% was added, and 0.24g of flux was added. Then heating and ultrasonic treatment for 30min at 50 ℃ under 200W, stirring uniformly, putting the solution containing graphite into a high-temperature furnace, pumping air to a reduced pressure state, keeping about 0.3atm in the first stage, and performing alkaline leaching under reduced pressure for 1.4h. Heating after alkaline leaching, maintaining the temperature at 200 ℃ and the pressure at 0.5-0.8atm, drying until the water volatilizes completely, alkaline-melting roasting at 500 ℃ for 120min, cooling to 50 ℃, magnetically stirring and leaching for 30min, filtering, washing to neutrality, and drying the filter cake. Adding the graphite after alkali fusion into 80mL of 1.5mol/L nitric acid solution, leaching for 80min at 80 ℃ to remove impurities in the graphite, filtering, washing to be neutral, and drying to obtain a finished product. The fixed carbon content of the graphite finished product reaches 99.96 percent.
Comparative example 2
The difference from example 2 is that: the fixed carbon content of the obtained graphite finished product is 99.28 percent without adopting reduced pressure alkali fusion.
Example 3
3.2g of sodium hydroxide is dissolved in 10mL of deionized water, and the mass ratio of graphite to sodium hydroxide in the prepared alkali liquor is 1:0.8 to 4g of graphite powder having a carbon content of 91% was added. Then heating and ultrasonic treatment for 30min at 50 ℃ under 200W, stirring uniformly, putting the solution containing graphite into a high-temperature furnace, pumping air to a reduced pressure state, keeping about 0.5atm in the first stage, and performing alkaline leaching under reduced pressure for 1.5h. Heating after alkaline leaching, maintaining the temperature at 200deg.C and pressure at 0.5-0.8atm, drying until the water volatilizes completely, alkaline-melting and roasting at 550deg.C for 120min, cooling to 50deg.C, magnetically stirring and leaching for 30min, filtering, washing to neutrality, and oven drying the filter cake. Adding the alkali-melted graphite into 80ml of 1.5mol/L nitric acid solution, leaching at 80 ℃ for 80min to remove impurities in the graphite, filtering, washing to be neutral, and drying to obtain a finished product. The fixed carbon content of the graphite finished product reaches 99.90 percent.
Comparative example 3
The difference from example 2 is that: the fixed carbon content of the obtained graphite finished product is 99.25% without adopting reduced pressure alkali fusion.
The principles and embodiments of the present invention have been described herein with reference to specific examples, the description of which is intended only to assist in understanding the methods of the present invention and the core ideas thereof; also, it is within the scope of the present invention to be modified by those of ordinary skill in the art in light of the present teachings. In view of the foregoing, this description should not be construed as limiting the invention.
Claims (8)
1. The method for purifying the reduced pressure alkali-melted graphite is characterized by comprising the following steps of:
(1) Adding graphite powder into a sodium hydroxide solution, heating, and then stirring by ultrasonic to enable graphite to fully contact with sodium hydroxide to obtain a mixture I;
(2) Placing the mixture I into a high-temperature furnace for air extraction and decompression, performing reduced pressure alkaline leaching, heating and drying until the moisture is completely volatilized after alkaline leaching, continuously heating and performing reduced pressure alkaline melting roasting, and washing the graphite subjected to reduced pressure alkaline melting with deionized water to be neutral to obtain a mixture II;
(3) And mixing the mixture II with acid liquor, carrying out acid leaching under the conditions of heating and stirring, carrying out suction filtration after the acid leaching is finished, recovering the acid liquor, washing a filter cake with water to be neutral, and drying to obtain the purified graphite.
2. The method for purifying reduced pressure alkali-melted graphite according to claim 1, wherein the concentration of the sodium hydroxide solution in the step (1) is 5wt% to 30wt%, and the weight ratio of the graphite powder to the sodium hydroxide is 1:0.6-1:0.8.
3. the method for purifying reduced pressure alkali-melted graphite according to claim 1, wherein the ultrasonic stirring temperature in the step (1) is 40-60 ℃, the ultrasonic stirring time is 15-90min, and the ultrasonic stirring power is 200W.
4. The method for purifying reduced pressure alkali-melted graphite according to claim 1, wherein the pressure of the alkali leaching in the step (2) is 0.3-0.5 atm, and the time of the alkali leaching is 0.5-1.5h.
5. The method for purifying a reduced pressure alkali-melted graphite according to claim 1, wherein the reduced pressure alkali-melted graphite in the step (2) has a reduced pressure alkali-melted baking temperature of 400-600 ℃, a reduced pressure alkali-melted baking pressure of 0.5-0.8atm, and a reduced pressure alkali-melted baking time of 1.5-3.0h.
6. The method for purifying the reduced pressure alkali-melted graphite according to claim 1, wherein the acid liquid in the step (3) is one or more of hydrochloric acid, nitric acid and sulfuric acid, and the concentration of the acid liquid is 1.5mol/L.
7. The method for purifying reduced pressure alkali-melted graphite according to claim 1, wherein in the step (3), the solid-to-liquid ratio of graphite to acid solution is 1g:20mL, the acid leaching temperature is 80 ℃, and the acid leaching time is 80min.
8. The method for purifying reduced pressure alkali-melted graphite according to claim 1, wherein the fixed carbon content of the purified graphite in the step (5) is not less than 99.9%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310060640.0A CN116040626B (en) | 2023-01-17 | 2023-01-17 | Method for purifying reduced pressure alkali fusion graphite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310060640.0A CN116040626B (en) | 2023-01-17 | 2023-01-17 | Method for purifying reduced pressure alkali fusion graphite |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116040626A true CN116040626A (en) | 2023-05-02 |
| CN116040626B CN116040626B (en) | 2024-05-28 |
Family
ID=86132929
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310060640.0A Active CN116040626B (en) | 2023-01-17 | 2023-01-17 | Method for purifying reduced pressure alkali fusion graphite |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116040626B (en) |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101920957A (en) * | 2010-08-17 | 2010-12-22 | 北京矿冶研究总院 | Preparation method of high-purity graphite |
| CN103265331A (en) * | 2013-05-22 | 2013-08-28 | 苏州赛菲集团有限公司 | C/SiC/Na2SiO3 antioxidative compound coating suitable for graphite material and preparation method thereof |
| CN107522197A (en) * | 2017-09-15 | 2017-12-29 | 福建翔丰华新能源材料有限公司 | The method of the preparation high-purity of economy, the micro crystal graphite of high graphitization degree |
| CN109320298A (en) * | 2018-10-17 | 2019-02-12 | 中国科学院山西煤炭化学研究所 | A method of improving foamy graphite surface wettability |
| CN111354939A (en) * | 2020-02-24 | 2020-06-30 | 广东东岛新能源股份有限公司 | Porous silicon composite material and preparation method and application thereof |
| CN113831139A (en) * | 2021-09-29 | 2021-12-24 | 湖北瑞宇空天高新技术有限公司 | C/SiC composite material for gas rudder of aerospace engine and preparation method thereof |
| JP7047239B1 (en) * | 2021-03-08 | 2022-04-05 | 株式会社レイホー製作所 | Manufacturing method of graphite material |
| CN114478068A (en) * | 2022-01-25 | 2022-05-13 | 江西宁和达新材料有限公司 | High-temperature oxidation-resistant graphite product and preparation method thereof |
| CN115092941A (en) * | 2022-07-11 | 2022-09-23 | 哈尔滨工业大学 | Method for recovering residual carbon and sodium silicate from coal gasification fine ash by using low-temperature alkali fusion method and application |
| CN115490230A (en) * | 2022-10-25 | 2022-12-20 | 苏州中材非金属矿工业设计研究院有限公司 | Efficient alkaline-acid purification system and process for graphite |
-
2023
- 2023-01-17 CN CN202310060640.0A patent/CN116040626B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101920957A (en) * | 2010-08-17 | 2010-12-22 | 北京矿冶研究总院 | Preparation method of high-purity graphite |
| CN103265331A (en) * | 2013-05-22 | 2013-08-28 | 苏州赛菲集团有限公司 | C/SiC/Na2SiO3 antioxidative compound coating suitable for graphite material and preparation method thereof |
| CN107522197A (en) * | 2017-09-15 | 2017-12-29 | 福建翔丰华新能源材料有限公司 | The method of the preparation high-purity of economy, the micro crystal graphite of high graphitization degree |
| CN109320298A (en) * | 2018-10-17 | 2019-02-12 | 中国科学院山西煤炭化学研究所 | A method of improving foamy graphite surface wettability |
| CN111354939A (en) * | 2020-02-24 | 2020-06-30 | 广东东岛新能源股份有限公司 | Porous silicon composite material and preparation method and application thereof |
| JP7047239B1 (en) * | 2021-03-08 | 2022-04-05 | 株式会社レイホー製作所 | Manufacturing method of graphite material |
| CN113831139A (en) * | 2021-09-29 | 2021-12-24 | 湖北瑞宇空天高新技术有限公司 | C/SiC composite material for gas rudder of aerospace engine and preparation method thereof |
| CN114478068A (en) * | 2022-01-25 | 2022-05-13 | 江西宁和达新材料有限公司 | High-temperature oxidation-resistant graphite product and preparation method thereof |
| CN115092941A (en) * | 2022-07-11 | 2022-09-23 | 哈尔滨工业大学 | Method for recovering residual carbon and sodium silicate from coal gasification fine ash by using low-temperature alkali fusion method and application |
| CN115490230A (en) * | 2022-10-25 | 2022-12-20 | 苏州中材非金属矿工业设计研究院有限公司 | Efficient alkaline-acid purification system and process for graphite |
Non-Patent Citations (1)
| Title |
|---|
| 王启立: "煤基多孔介质的表征、流动及应用", 29 February 2020, 中国矿业大学出版社, pages: 15 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN116040626B (en) | 2024-05-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106848472A (en) | A kind of method that lithium is reclaimed in waste lithium iron phosphate battery | |
| CN109868364A (en) | A kind of waste lithium cell wet process line recovery method | |
| Wu et al. | Selective recovery of lithium from spent lithium iron phosphate batteries using oxidation pressure sulfuric acid leaching system | |
| CN110589812A (en) | Method for preparing porous graphene by recovering graphite cathode material from waste power battery | |
| WO2021244189A1 (en) | Method for graphite purification and lattice reconstruction in power battery | |
| CN110620277A (en) | Method for separating and recovering valuable metal from waste lithium ion battery anode material | |
| CN115287469B (en) | Method for selectively extracting lithium from clay-type lithium ore | |
| CN112047335A (en) | Combined treatment method for black powder of waste lithium ion battery | |
| CN114335781A (en) | Method for extracting precious metal from waste lithium battery | |
| CN114394610A (en) | Recovery method of waste lithium iron phosphate battery | |
| CN116040626B (en) | Method for purifying reduced pressure alkali fusion graphite | |
| GB2623222A (en) | Method for extracting lithium from waste lithium battery | |
| CN113206227A (en) | Method for preparing carbon-based metal sulfide negative electrode material by simultaneously recycling positive and negative electrode materials of waste nickel-cobalt-manganese lithium ion battery | |
| CN114229812A (en) | Method for extracting iron and phosphorus from lithium iron phosphate waste | |
| CN109616668A (en) | The micro- preparation method for expanding layer natural graphite of lithium cell negative pole material manganese oxide-small size | |
| CN109346716A (en) | A kind of method that non-wood papermaking raw material alkali process waste liquid prepares C/SiOx composite lithium ion battery negative electrode material | |
| CN115304059B (en) | Recycling treatment method for retired battery carbon residue | |
| CN114408916B (en) | Expanded graphite and preparation method thereof | |
| CN103326022A (en) | Method for preparing lithium ferrous silicate positive pole material from ilmenite | |
| CN110699552B (en) | Method for selectively extracting high-purity metal titanium from SCR catalyst | |
| CN109876862B (en) | Preparation method and application of composite photocatalytic material | |
| US20240239664A1 (en) | Expanded graphite and preparation method therefor | |
| CN116282080B (en) | Continuous freezing production process of sodium sulfate in waste lithium iron phosphate battery recovery process | |
| CN114229855A (en) | Method for extracting mesoporous silica from fly ash by utilizing boron oxide circulating phase separation | |
| CN110523751B (en) | Method for recycling carbon substances in waste cathode leaching residues of aluminum electrolysis cell |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |